Manufacture of plastic molding powders



Patented July 26, 1949 MANUFACTURE F PLASTIC lilOLDING POWDERS Jack Sandler, South Orange, N. J., assignor to Hungerford Plastics Corporation, New Providence, N. J., a corporation of New Jersey Application January 1a, 194s, sei-m No. 642382 2z claims. (ci. 10s-19s) This application is a continuation in part of my abandoned application Serial No. 578,111 filed February 15, 1945.

The present invention relates to the conditioning of solid materials in particle form and has particular reference to the conditioning of organic materials in such form which require treatment involving the addition of other material in fluid form in order to be converted into a molding material in particle form capable of being transformed by the application of heat and pressure into a cohesive solid product. Still more particularly, the invention relates to the conditioning of materials such as cellulose derivatives, vinyl polymers and other resins, and other plasticizable material requiring the addition of plasticizer and/or other organic material and in some instances the removal of volatiles in order to produce a material in particle form capable of formation into plastic bodies by heat and pressure. For convenience, the material produced by the present invention will herein be referred to generically as molding material, this term being intended to include materials suitable for subsequent application of heat and pressure by extrusion, injection, calendering, casting and like operations, which will be referred to generally as molding.

The material from which desired molding materials are made and which may for example but without limitation be a cellulose derivative, a resin or other suitable plasticizable material, is ordinarily supplied by the manufacturer in powder or flake form, the particle size of which may vary widely from relatively coarse sand-like granular or even fibrous condition to relatively very fine dust-like powder. For the purpose of this specication, such material will be referred to generally as material in particle form.

Such material, depending upon its nature and the nature of the use to which the end product is to be put, may require one of a number of different treatments to condition it for molding. One of the commonest of the treatments required is the addition of a plasticizer which in most instances is a liquid and which must be uniformly distributed so that each particle of the material is placticized if a high quality molded product free from iiaws is to be obtained. In addition, it is in many instances desirable to add a colorant which may be in either powder or liquid form, inert solid filler which ordinarily is in particle form, so-called stabilizers, inhibitors, lubricants and other extraneous materials, and it is further necessary in certain instances to remove from 2 the particle material volatiles such as residual solvents employed inproducing it and moisture which the material may have absorbed from the atmosphere. Certain of the conditioning materials which it may be desired to add to the particle material before molding may be adsorbed or absorbed, while others may desirably be only for the purpose of providing a uniformly distributed coating on the particles of the mass of material.

The general object of the present invention is the provision of new and improved methods of processing material of the character under consideration, particularly so as to condition it to produce the desired kind of solid article by subsequent molding operations. Other and more detailed objects of the invention together with the advantages to be derived from its use will appear as this specification proceeds.

In accordance with methods heretofore employed for conditioning material to produce a suitable molding powder, the material in particle form is in most instances dissolved in a suitable solvent to form a colloidal gel-like mass to which a desired added material such for example as plasticizer i-s added in particle and/or liquid form. This mass of material is then mechanically mixed or kneaded to effect the desired preliminary blending or colloiding and is then worked on heated converting rolls which operate further to blend the materials and which also may drive on a part of the solvent used to produce the mass. After this operation, the resultant strips or slabs of material are then mechanically disintegrated to again form solid material in particle form which after moisture and all remaining solvent is removed is suitable for subsequent molding operations.

The above generally outlined method is relatively slow and expensive and requires the use of machinery which is heavy and expensive in relation to its capacity to produce finished material. Also, in some instances the quality of the product is impaired because of degradation resulting from relatively high temperatures to which the material must be subjected during the processing.

Recognizing the deficiencies of the general procedure above discussed, it has heretofore been proposed to effect the desired conditioning of such material without reducing it to a dough-like mass during the process, such methods involving the use of additional fluids later removed from the end product, so that the processes can be classified generally as wet processes. These latter processes have, however, not proved to be arranco commercially practicalgavnd the processing still generally employed is that which involves reducing the material to a dough-like mass, treating it in such form, and then mechanically disintegrating the mass after it has been solidied.

The present invention, on the other hand, contemplates the conditioning of the material to be treated by what may be termed an essentially jdry process in which the particle material is maintained throughout the process in substantially dryfstate even though the conditioning process requires. the addition of material in iuid form to the mass of particle material, the required uniformity of distribution of the fluid throughout the mass being accomplished by treatment hereinafter explained. l

For the purpose of this specification and the appended claims, the terms essentially dry or substantially dry as applied to the process and/or the material are to be understood as meaning that degree of dryness which results in the mass oi' material Ibeing treated remaining in substantially free-flowing condition in its particle form, in contrast with an agglomerated mass.

To this end, theprocess contemplates agitating the mass of particle material in substantially dry state and while maintaining it in that state adding and/or removing from the particle material the other materials required in order to condition the material to produce the desired end product, such additions and/or removals being carried out under conditions of temperature and pressure and at controlled rates such as toavoid agglomeration of the mass and further so as to insure uniformity of conditioning.

The preferred manner in which the process is carried out is by tumbling the massto be treated in a closed rotary tumbling vessel and intro- -ducing the material which is required to be added in uid form, by injection at a rate and soy controlled in relation to the rotation of the blending vessel that the particles of the mass being treat- 'ed are exposed a multiplicity of times to the material being introduced, the desired uniform distribution of the added material being effected by the combination of the repetitive direct addition of relatively small quantities of added fluid and the rubbing contact over a. substantial period of time between the particles of the mass moving relative to each other in their free-flowing state.

In order better to understand the more detailed nature of the invention and the manner in which its principles may be employed to effect its several objects, reference may best be had tothe ensuing portion of thisspecification taken in conjunction with the accompanying drawings which illustrate in purely diagrammatic form ap- *paratus suitable for carrying the invention into -eect.

In the drawings, Fig.l 1 isa view illustrating 'conditioning apparatus capable'of carrying the' invention into effect, Fig. 2 is a section taken on the line 2-2 of Fig. 1, Fig. 3 is a section on enlarged scale of part of the apparatus shown in Fig. 1, and Fig. 4 is a section taken on line 4-4 of Fig. 3 showing the contour of a .cam forming a 'part of the apparatus.

Referring now tothe drawings, I have-shown more or less diagrammatically in Fig. 1 apparatus capable of carrying into eiect the principles signed to be limited to a particular treatment of a specific material.

In the apparatus illustrated, a rotary mechanical blender I of the tumbling type is provided, the blender advantageously but not necessarily being of the kind comprising two frusto-conical parts l2 joined by a cylindrical central section is, with the larger or base diameters of the conical parts in confronting relation. The blender is mounted on suitable trunnions I6 and I8 to rotate about the axis which is preferably horizontal. In the embodiment illustrated the small end of one of lthe conical portions is closed by means of a cover 22, shown hinged to permit charging v and removal of a batch of material from the vessel. The vessel is further provided with means pervious to a gaseous iluid but impervious to the solid contents of the vessel, for permitting the escape from the vessel of gaseous iluid whichk may be introduced into the vessel during the processing of the material. In the embodiment illustrated. this is effected by utilizing a cover 24 of porous=.metal, such as that made by powder in a nozzle or jet orifice 28 located in the central region voi? the vessel. Conditioning material to be applied in fiuid form to the mass ofy particle material within the vessel is injectedffrom a reservoir or receptacle 30. Air or gas under pressure is supplied through pipe 32 under control of the valve to this receptacle for forcing liquid from the receptacle 'through' a discharge pipe 3d controlled by valve 36 and leading to a tube 38 having anforifice 40 at its inner end. Air or gas is supplied to the -outer tube 26 through conduit 42 and, as will be evident from the drawing, when pressure is supplied to the receptacle andvalve 36 is opened the pressure will force a stream .of liquid through `the opening 40 where it will be mixed with the gaseous uid under pressure in tube 2B and discharged in jet form through the orifice '28. Depending upon factors hereinafter discussed, the form ofthe fluid as discharged may be as a solid stream ordrops of liquid,v a coarse or a ilner spray, or a vapor, to all'of which forms the term jet may be generically applied.

While in the accompanying diagrammatic i1- lustration, injection of fluid has been indicated as being accomplished lby means of apparatus having only `a single injection orifice and utilizing a gaseous medium as an atomizing agent, practice of the invention isy not'limited to such apparatus vsince in some instances it may be desirable to employ vamplu'ralitvy of such orifices and it may also be sumcient' when spray injection is desired to employ other'known forms of injection apparatus of the kindinfwhich a spray is produced by high liquid pressure alone which is released through a suitable Jet'oriiice. as in the case of injection nozzles 'for Diesel engines.

As 'previously noted,4the method contemplated by the present invention is essentially a dry method which maintains the particle mass linfrecilowing condition during the process. To this end,v the fluidintroduced into the blendingv vessel mustbe controlled as to rate and manner of introduction so as to avoid appreciable wetting o! the wall of the vessel since if that occurs agglomeration or lumping of the particle material ensues. To avoid such wetting, the fluid material is introduced into the vessel so that direct contact is substantially entirely between the introduced fluid and the mass oi particle material in the vessel.

To this end. when a tumbling vessel oi the kind herein illustrated is employed and additional iiuid material is injected, the jet is advantageously directed angularly, as indicated at 2l in' Ii'ig. 2, so as to be directed toward the upwardly moving or rising side of the vessel, the direction of rotation of the vessel in Fig. 2 being in the direction indicated by the arrow a. In a vessel of the kind illustrated, the material is carried upwardly along the rising side of the vessel as it rotates and injection in such case in the direction indicated will cause the injected iiuid to be directed substantially only toward a part of the vessel where the wall is covered by a mass of the particle material and moreover toward a part of the vessel where.

to the rotation of the vessel, in order to avoid' appreciable wetting of the wall of the vessel. In the embodiment illustrated, this is accomplished by opening valve 36 in timed cycle relation bymeans of a cam 42, the contour of which is so shaped that the valve is opened at those times in the cycle when the resultant spray will be directed substantially only against the mass of material in the vessel.

The cam illustrated provides two injection periods per revolution of the vessel but it will be understood that in the case of large vessels or forms of blending vessels other than that illustrated, different numbers and timings of injection periods may be employed. Usually, a plurality of injections per revolution of the blending vessel will be employed but in certain instances where relatively small percentages of fluid are to be added this may not be the case, for reasons hereinafter pointed out. An important criterion is avoidance of wetting the wall of the vessel to an extent resulting in substantial agglomeration of the particle material.

In cases where injection is effected by the aid of a gaseous medium, the air or gas for this purpose, and for other purposes hereinafter to be described, is supplied from a suitable pump (not shown) or pressure line 48 to a drier containing a mass 50 'of suitable material for absorbing moisture, such for example as activated alumina, for removing at least the greater portion or all of the moisture from the medium supplied to the blending vessel. A conduit 52 in which there is advantageously provided a control valve 54 leads to a heater 56 which may be supplied with heat from any suitable source, such source being diagrammatically illustrated by the burner 58. A conduit 60 connects the outlet of the heater 56 to the tube l2 entering the blender through the hollow trunnion i6, this conduit advantageously being provided with a control valve 6l. The conduit I2 leading to the receptacle 3|! supplying the injection apparatus is connected under the control of valve 88 to the outlet side of the drier 48 and through a by-pass conduit 68 and control valve 10 is also connected to the outlet of the 6 heater Il. Conduit l2 is connected through the branch conduit l2 advantageously under the control ot valve to the tube 2l of the injection apparatus and is further connected by a branch. controlled by valve Il, to the conduit lll. Conduits 32 and il are further advantageously supplied with control valves 83 and l5 respectively.

For certain kinds of processing within the scope of the invention, the receptacle 30 is advantageously heated as by means of the burner indicated at Il and also may have provided therein some means for agitating the uid contents as by means of the mechanical agitator indicated diagrammatically at 35. Further, the connection for carrying the iiuid from receptacle 30 to the oriiice through which it is injected into the blending vessel may be heated as indicated diagrammatically by the heating coil 31 around the pipes Il, 3l.

Other processing contemplated /may require limitation 'of the temperature attained by the mass of particle material and for this purpose the conduit 60 may advantageously be provided with cooling means indicated by the cooling jacket I1 through which a suitable cooling i'iuid or refrigerant may be passed from inlet 69 to outlet 'I I.

The apparatus just described may within the purview of the invention be operated in a number of speciiic ways, depending upon the nature of the materials to be compounded and diierent specic aspects of the invention may best be understood by examples of which a few represen-A tative illustrative cases will be given.

Let it first be assumed that it is desired to produce a batch of uncolored molding powder the base of which is cellulose acetate ake requiring the addition of a relatively large amount of plasticizer. Let it further be assumed that a batch of pounds of such flake is to be plasticized by the addition of a suitable plasticizer such as a mixture of dimethyl and diethyl phthalate in the amount of 47 pounds.

With so much plasticizer to be added to the flake, the principal factor to be guarded against its agglomeration of the mass and to this end it is necessary that the fluid be introduced so that it does not impinge directly on bare Wall surface of the vessel and also the rate at which the iiuid is fed must be governed so that the tumbling action of the material has ample opportunity to distribute the introduced fluid as it is added.

I have found from experience that when the fluid is added so as to avoid any substantial direct impingement against the walls of the vessel and with a vessel of the kind illustrated being operated at a speed of 20-25 R. P. M., a rate of feed of the fluid material of approximately 0.8 of a pound per minute will operate to uniformly plasticize a batch of material such as that described above without harmful agglomeration thereof and with the material remaining in its substantially dry, free-flowing particle condition.

In some instances, it may be desirable to add relatively very small quantities of iiuid conditioning material and in such cases, the primary criterion of the rate oi' feed is the securing of uniform and thorough distribution throughout the mass of particle material of a relatively very small quantity of added fluid material. An example of this is in the production of so-called monofilament from a vinyl resin where it may be desirable to add as little as two pounds of stabilizer and lubricant in iluid form, such for example as tin soap and modiiied castor oil, to a one hundred pound batch of particle material. In such a case, I have found that with a blendlng vessel of the type illustrated, rotated at 20,-25- R. l. M., entirelysatistactory uniformity of; distribution is obtainable with a rate of feed of approximately 0.2 pound a minute. Where the rate of feed is so low and an intermittent feedis employed, the number of feeding or injection periods per revolution of the vessel may be one or .even less in contrast with the plurality of injections usually employed when a relatively large amount of -fluid conditioning material is to be added.

Insofar as the control of the rate of feed oi added uid is concerned, this may be accomplished in numerous diierent ways in addition to the number of injections per-revolution when intermittent injection is employed, as for example by the height of the lift of a cam operating an imection control valve and/or control of the pressure at whichthe liquidand/or gas is admitted tothe injection apparatus, so vas to control the rate of iiow of the fluid during the period of admission whether such period be continuous or intermittent.v

l The rate of feed is, however, so related to the speed of revolution of the blending vessel that the mass of base material is tumbled a multiplicity of times during the compounding periodso that in, effect the added fluid is directed against rubbing contact between the particles within the -vinyl chloride acetate and vinyl acetate.

tumbled mass.

phthalata tricresylA phosphate, triphenyl phosphate, diethyl sebacate, sucrose octa acetate. dlr methoxyli ethyl phthalate, dimethyl phthalate, diethyl phthalate, diphenyl mono-o-xenyl phostate, lubricants such asstearic acid, zinc stearate and various oleates, and solid fillers such as carbon black, calcium carbonate or other such materials', may be employed insecuring the .lesired end products.

The process is also applicable in the' oase of bitumens where for example a bitumen of asphalt nature may bel compounded with a filler such as clay and a colorant and conditioned subsequently In the event it is desired to employ a colorant.-

4 with -the particle material to be coloredv and blended therewith by tumbling action prior to or concomitantly with the addition of the iluid conditioning material. Alternatively, such la colorant may be reduced to-fluid form by a suitable solvent whichis not a solvent for the particle material and introduced in liquid form in the same manner as other iiuid conditioning materials, the solvent later being removed as hereinafter described. If the colorant is naturally in liquid form, it obviously may be added in the same manner as other iluid conditioning materials. One or another of the procedures outlined above may also be employed in cases where it is desirable to add other conditioning materials, inclusive of illlers, plasticizers, inhibitors, lubricants or the like, which may be naturally in soild form. f i

The process is applicable in its different as pects to a wide-variety of basic products for conditioning to produce a large number of diilerent specificl end products. It is well adapted for plasticizing materials such as cellulosic derivatives and the polymeric plastics such as the vinyl polymers requiring plasticization, coloring or other conditioning treatment, including among such materials but without limitation cellulose derivatives such as cellulose acetate, cellulose acetate butyrate, cellulose acetate propionate, cellulose triacetate, ethyl cellulose andbenzyl ce1lulose,landpolymers such as vinyl chloride,

Applicable plasticizers for such materials include acetyl triethyl citrate, methyl phthalyl ethyl glycolate, ethyl phthalyl ethyl glycoiate, butyl phthalyl ethyl glycoiate, glycerol triacetate, di-

methyl phthalate, diethyl phthalate, dibutyl for subsequent molding by 'the addition of a liquid such as gilsonite subsequently acting as a bonding agent. I

In come cases, the conditioning may involve, in addition to compounding, the removal of certain residual undesirable volatiles from the particle material being treated, as for example in the case where it may be desirable to add color to methyl methacrylate-in particle form and remove from it residual volatiles and/or moisture.

Still another instance of the utility of the process is coating of a particle material with a conditioning material which normally is in solid form, as for example the treatment of 'a material in particle form such as polyethylene, the particles of which it may be desired to condition with a thin film coating of a wax.

As is well-known, it is essential to successful molding thatmoisture must be substantially entirelyremoved from molding powder before heat and pressure are applied to form the desired article. Many of the materials employed, of

which cellulose acetate is an example, absorb suilicient moisture from the atmosphere to which they have been exposed to require drying in order to' produce a suitable molding powder. The present invention includes among other things the drying of the material within the blending vessel to a degree rendering it suitable for immediate molding without further drying treatment. This may be accomplished by employing dried air, which may also be heated, as the carrier fluid for spraying injected liquid vand/or by introducing such a-ir separately into the vessel4 before, during or after the compounding phase of the cycle. By proper manipulation of suitablecontrol valves, it will be apparent that the desired cycle may be carried out in numerous differentspecic ways, as for instance by a predrying period of the material before compounding .with an added conditioning fluid followed by a compounding period and further followed by a second drying period 'during which moisture and/or solvents for the conditioning material may be driven off. l f

The apparatusdiagrammatically illustrated herein is illustrative of the many variations that can be carried out and while for the sakeofsim-y plicity manually operated valves have been shown, it will readily be seen that automatically timed control valves ofknown construction may be employed for manipulation so that the selected control oi specinc sequences oi'. events can be accomplished automatically.

By way of example, let it be assumed that it is .desired to plasticize and dry a material such as cellulose acetate, using a plasticizer naturally in liquid form. In such case, the liquid is placed in vessellli and the compoundingeii'ected by air dried in vessel 4I and admitted to the injection apparatus through conduit 32, valves 54, Il and 'I0 being closed, heat not being required in order to eil'ect the injection of the liquid plasticizer. After the compounding period is completed, the material may be then thoroughly dried by heated air admitted through the pipe I2, valve Il being closed and valves M and 84 being opened to per-v mit now of the air from the heater 5l to the blending vessel.

In cases, for example, where the conditioning material to be added in fluid form requires heatinglto convert it into such form from its naturally solid state, the conditioning material may be placed in the vessel 30 and heated by burner 3i or other source of heat, and also mechanically agitated, particularly in cases where the conditioning material as injected is composed of different substances blended together before being delivered to the blending vessel. In order to avoid re-solidication ci 'such material, the ln- Jection apparatus may also be advantageously kept heated as by means of the heating coil 31. Also in such cases, it will usually be desirable to employ heated air if gaseous injection is employed and in such case, the valves I4 and 'l0 may be opened so as to supply heated air to the injection apparatus. During such a compounding process, it may further be desirable to supply additional heated air to the mass oi particle material so as to prevent premature re-solidincation of the conditioning material when it strikes the material to be conditioned. Some materials which it may be desired to treat may soften at relatively low temperatures and in some instances it may be'desirable to treat such materials with a conditioning material that can be converted to fluid form only by heating to a temperature approaching or even exceeding the temperature at which the material to be treated would soften. Even in such cases, the present process can be employed to effect the desired treatment by limiting the temperature of the mass of particle material by cooling it as the hot liquid is applied. In the apparatus illustrated, such a procedure may be accomplished by heating the fluid in the container 30, utilizing heated air if desired as a carrier for the injection apparatus by opening valves 54 and 10, while simultaneously introducing cold air into the blending vessel by opening valves 68, 6| and 64, valves 63 and 85 being closed. If required, the cooling air may be refrigerated as by the cooling jacket ,81, through which a suitable coolant or refrigerant is circulated from inlet 89 to outlet 1I.

From the foregoing examples, it will be apparent that the process is, in its various aspects, of widely varied utility and it further will be apparent that, depending upon the specific materials to be treated and end products desired, certain features hereinbefore described may be employed to the exclusion of others. As will likewise be apparent, fluid conditioning material may be added within the scope of the invention to a mass of particle material comprising only a single constituent such as raw acetate or vinyl powder or to a composite mass in particle form comprising a blended mixture of different constituents. Such particle material, whether consisting of one or more constituent materials, will be referred to herein generally as base material.

' steps and to this end the blender may advantageously be located so that the finished material as discharged from the blender may be fed directly to asuitable molding machine. This arrangement is diagrammatically indicated by an extrusion molding machine shown generally at 12. The specific form of the molding machine is not germane to the present invention and for purposes of illustration there is shown an ordinary type of extrusion molding machine having a hopper 14 with a slide cover 16 and delivering to a pressure chamber i8 in which is located a variable pitch screw driven from any suitable source of power indicated by the gearing 8l. 'Ihe pressure chamber is advantageously heated by any suitable means such as the electric heating element indicated at 82 and the material is delivered from the pressure chamber 18 to the extrusion die 8l which forms the molded product 86 to the desired configuration.

In addition to being productive of the numerous advantages previously enumerated, the present invention, is productive of a superior quality of product. Due to the fact that the conditioning of the material is carried out ata low temperature level and without the application of appreciable pressure, no degradation of the material is caused by these factors. In contrast with the material produced by the presently commonly employed methods, the particle material or powder produced by the present invention is in what may be said to.be non-homogeneous form inwhich the constituents of the material, which may for example consist of a base material, plasticizer and color, have not undergone any chemical change as a result of the conditioning process, and while thoroughly and uniformly distributed, are not converted into a homogeneous mass until the application for the vfirst time of substantial heat and pressure in the actual molding operation.

As will be apparent from the foregoing description, the invention in its several aspects has a wide eld of utility applicable to many different specific -materials and combinations thereof to produce many different kinds of desired end products. The invention is accordingly r to be understood as not limited to the specific examples herein given by way of illustration but is to be construed as limited only by the scope of Athe appended claims.

What is claimed: 1. The method of making molding material in particle form capable of being transformed into a cohesive solid product by application of heat and pressure which includes the steps of tumbling a mass of base material in substantially dry particle form to bring diil'erent particles to the surface of the mass and applying a conditioning material iniluid form to the surface of the mass while the mass is being tumbled at a rate so related to the rate of tumbling of the mass that the mass is tumbled a multiplicity of times during the period of such application to change the surface layer of the mass a multiplicity oi times and maintain the mass in its substantially dry particle form, whereby to effect substantially uni'- form distribution of the added fluid throughout v11 Y 1 the substantially mass due to such `Vapplication of thel fluid to differently constituted surlface layers at diierent times andthe rubbing contact between the'particlesv ofthe mass during. said period. f i i 2. The method of making molding material-in particle form capable-oilbeingtransformed into v a cohesive solid product byy application of heat and pressure which includes the-steps of tumfl bling a mass of basematerial insubstantially dry particle form yto bring` different Aparticles of the surface of the mass'and applying a conditioning material in fluid form-tothe mass by spraying the applied materialon to thesurface of the mass while the mass is being tumbled at a rate yso re 3. The method of making mening material in particle form capable of being transformed into a cohesive solid product by-applicatio'riv of heat and pressure which includes the steps of tumbling a mass of base material in substantially dry particle form to bring diilerent particles to the surent particles to the of the mass and appiying a conditioning material'comprising a suitableplasticizer in fluid form to the surface of the mass while the mass is being tumbled at a raie so related to the rate of tumbling ofthe massl that the mass is tumbled a multiplicity of times during thel period of such application to change the'surface layei. o f the mass a multiplicity of times and maintain the massY in yits substantially dry parti-4 cle'form.- whereby to eii'ect substantially-uniform distribution of th'eAadded iiuid through the substantially dry mass due to such-applicationof the iiuid to' Adifferently constituted surface layers at diiferent times andthe rubbing contact between the particles of the mass 'during said period.

6. The method of making molding material in particle form capable of being transformed into a cohesive solid product'byapplication of, heat and pressure which include'sth'e steps of tumblingin substantially dry particle forma mass of material comprising ya. polymeric vplastic requiring plasticizing, whereby to bring different particles to the.

surface of themass. and applying aconditioning material comprisinga suitable vplasticizer in fluid form to the surface of the mass while the mass is being tumbled at a rateso related to the rate of tumbling of the massjthat the'mass is tumbled a face of the mass and intermittently applyingV a conditioning material in fluid. form tothe surface of the mass while the mass lis being tumbled at a rate so related to the rate of tumbling of the mass multiplicity -of times during the periodo! such application to change the surface layer of the mass a multiplicity of times and lmaintain the mass in its substantially dry particle form. whereby to effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the fluid to differently constituted Asurface 'layers at different timesr and the rubbing contact between the lparticles of the massdurng said period.

that the mass is tumbled a multiplicity oi.' times during the period of such application to change the surface layer of the mass a `multiplicity of times and maintain the mass in its' substantially vdry particle form, whereby to eiIect substantially uniform distribution of the added fluid throughout the substantially drymass due to such application of the fluid to differently constituted sur-v face layers at different times and therubbing contact between the particles ofthe mass during said period. 1

4. The method of malring molding material in particle form capable of being transformed into a cohesive solid product byapplication of .heat

7. 'The method of xnakingmolding material in particle form capable of being transformed into of the mass a multiplicity of times and maintain and pressure which includes vthe steps of tumbling in substantially dry particle form amass oi organic material requiring the addition of a plas` ticizer, whereby to bring different particles to the surface of the mass, and applying an organic plasticizer in iiuid form to the surfaceofthe mass while the mass is being tumbled at ajrate so r e" lated to the rate of tumbling -of the mass v that the mass is' tumbled a multiplicity of times during the.

5 whereby to effect substantially uniform distribu period of such application to change the surface layer of the mass a multiplicity of. ',times and maintain the mass in its substantially parti` cleform, whereby to effect substantially uniform distribution of the added fluid throughoutthe substantially dry mass due to such application of the fluid vto differently constituted `surface lay-` ers at diierent times and the rubbing contact be.- tween the particles of themass during said period.

5. .'Ihe -method of making molding materialin particle form capable of being transformed into a cohesive soliciy product by application of -heat and pressure which includes the steps of tumbling. in substantially dry particle form a mass of material comprising a cellulose derivative to bring dinera cohesive solid product by application of 4heat and pressure which includes the steps of tumbling a mass of basematerialin substantially dry particle form to bring different lparticles tothe surlface of the mass, heating a conditioning material and applying the heated-conditioning material in fluid form to the surface of the mass while the massjis being tumbled at a rate so related to the rate'oftumbling of the mass v,that the mass is tumbled a multiplicity of times during the periodv of l suchl application to change the surfacejlayer the mass inits substantially dry particle form,

tion of the added fluid throughout the substan tially dry mass due4 to such application of the fluid to diilerently constituted surface layers v at different times and'the'rubbingcontact between the particles of the mass during said period.y

8. The method'of making molding materialin particle form-capable' of'beingy transformed into a'cohesive'solid product by' application of heat and pressure lwhich includes the steps oi' tumbling a. mass of Abase material in /substantially -dry particle `-form to bring different particles to the surface of the `mass-,*applying a conditioning material in iiuid form to the surface of the mass while` themass is being tumbled at a rate so relatedto' the rate of tumbling ofthe mass that l they mass is tumbled a multiplicity of times 'during the period of vsuch application to change the ,surface layer of the mass a multiplicity of times and maintain the mass in its substantially dry 'particle form and applying heat to the mass ofk particle material while the conditioning material is beingapplied, whereby to effect substantially 13 uniform distribution of the added fluid throughout the substantially dry mass due to 4such application of the fluid to differently constituted surface layers at different times and the rubbing contact between the particles of the mass during said period.

9. The method of making molding material in particle form capable of being transformed into a cohesive solid product by application of heat and pressure which includes the steps of confining in a vessel and tumbling therein a mass of base material in substantially dry particle form to bring different particles to the surface of the mass, applying a conditioning material in fluid form to the surface of the mass while the mass is being tumbled at a rate so related to the rate of tumbling of the -mass that the mass is tumbled a multiplicity of times during the period of such application to change the surface layer of the mass a multiplicity of times and maintain the mass in its substantially dry particle form, and passing a gaseous medium through said vessel to remove volatiles from the mass whereby to effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the duid to differently constituted surface layers at different times and the rubbing contact between the particles of the mass during said period.

10. The method of making molding material in particle form capable of being transformed into a cohesive solid product by application of heat and pressure which includes the steps of confining in a Vessel and tumbling therein a mass of base material in substantially dry particle form to bring different particles to the surface of the mass, applying a conditioning material in fluid form to the surface of the mass while the mass is being tumbled at a rate so related to the rate of tumbling of the mass that the mass is tumbled a multiplicity of times during the period of such application to change the surface layer of the mass a multiplicity of times and maintain the mass in its substantially dry particle form, and passing a heated gaseous medium through said vessel to remove volatiles from the mass whereby to'effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers at different times and the rubbing contact between the particles of the mass during said period.

11. 'I'he method of making molding material in particle form capable of being transformed into a cohesive solid product by application of heat and pressure which includes the steps of tumbling a mass of base material in substantially dry particle form to bring different particles to the surface of the mass, applying a heated conditioning material in fluid form to the surface of the mass while the mass is being tumbled at a rate so related to the rate of tumbling of the mass that the mass is tumbled a multiplicity of times during the period of such application to change the surface layer of the mass a multiplicity of times and maintain the mass in its substantially dry particle form and cooling the mass of particle material during said period of application, whereby to prevent softening of the particle material due to the application of the hot conditioning material and to effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the fluid to differently con- 14 stituted surface layers at' different times and the rubbing contact between the particles of the mass during said period.

12. The Amethodv of making molding material in particle form capable of being transformed into 'a cohesive solid product by application of heat and pressure which includes the steps of tumbling a mass of base material in substantially dry particle form to bring different particles to the surface of the mass, adding a colorant to the particle material and applying a conditioning material in fluid form to the surface of the mass while the mass is being tumbled at a rate so related to the rate of tumbling of the mass that the mass is tumbled a multiplicity of times during the period of such application to change the surface layer of the mass a multiplicity of times and maintain the mass in its substantially dry particle form, whereby to effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers at different times and the rubbing contact between the particles of the mass during said period,

13. The method of making molding material in particle form capable of being transformed into a cohesive solid product' by application of heat and pressure which includes the steps of tumbling a mass of base material in substantially dry particle form to bring different particles to the surface of the mass. mixing a colorant with other conditioning material and adding the mixture in fluid form to the surface of the mass while the mass is being tumbled at a rate so related to the' rate of tumbling of the mass that the mass is tumbled a multiplicity of times during the period of such application to change the surface layer of the mass a multiplicity of times and maintain the mass in its substantially dry particle form, whereby to effect substantially uniform distribution of the added fluid' throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers at different times and the rubbing contact between the particles of the mass during said period.

14. 'Ihe method of making molding material in particle form capable of being transformed into a cohesive solid product by application of heat and pressure which includes the steps of placing a mass of base material in substantially dry particle form in a rotatable blending vessel, rotating the vessel to agitate the mass to bring different particles to the surface of the mass and intermittently applying in timed relation to the rotation of the vessel a conditioning material in fluid form to the surface of the mass at a rate so limited that the mass is maintained in its substantially dry particle form and the surface layer of the mass changes a multiplicity of times during the period of such Iapplication, whereby to effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers at different times and the rubbing contact between the particles of the mass during said period.

15. The method of making molding material in particle form capable of being transformed into a, cohesive solid product by application of heat and pressure which includes the steps of placing a mass oi' base material in substantially dry particle form in a rotatable blending vessel.

'I5 rotating the vessel to agita-te the mass to bring material in fluid form to the surface of the mass 4 at a rate so limited that the mass is maintained in its substantially dry particle form and ythe vessel i's'rotated a multiplicity of times during the period required to inject the desired amountof conditioning material to thereby change the sur- 'face layer of the mass a multiplicity of times during said period, whereby to effect substantially uniform distribution of the added fluid Ithroughout the substantially dry mass due to such application of the fluid to differently constituted surface'layers at dierent times *and the rubbing contact between the particles of the mass during said period.

16`. The method of making molding material in particle form capable of being transformed `into a cohesive solid product by applicationof heat and pressure which includesthe steps of placing a mass of base material in substantially dry particle form in a rotating tumbling vessel, rotating thevessel to agitateA the mass to bring different particles to the surface of the mass and applying a conditioning material in fluid formto the surface of the mass byl injecting the conditioning material toward the rising side of the 'rotating vessel at a rate so limited that the mass is maintained in its substantially dry particle form and the surface layer of the mass changes a. multiplicity of times during the period of such application, whereby to effect substantially uniform distribution of the added fluid throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers at different times and the rubbing c on` tact between the particles of the mass during said period.

17. The method of making molding material in particle form capable of being transformed into a cohesive solid product by application of heat and pressure which includes the steps of confining a mass of base material in substantially dry particle form in a suitable vessel, agitating the mass to bring different particles to the surface y of the mass, applying a conditioning materialin fluid -form to the surface ofthe mass at =a rate so limited that the mass is maintained in its substantially dry particle form and the surface layer of the mass changes a multiplicity of times during the period of such application, whereby to effect substantially uniform distribution of the added uid throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers at different times and the rubbing contact between the par-ticles of the mass during said period, continuing the agitation of the mass of particle material after the conditioning material has been addedv and removing volatiles from the material by passing a gaseous medium through the vessel in which thematerial is confined. i

18. The method of making molding material in particle form capable of being transformed into a cohesive solid'product byI application of heat and pressure which includes the steps of confining a mass of base material in substantially layer of the mass changes a multiplicity of times during the periodoi.' such application, whereby to effect substantially uniform distribution of the added uid throughout the substantially dry mass due to such application of the fluid to differently constituted surface layers Iat 'different times and the rubbingcontact between 'the particles of the mass during said period, continuing the agitation of, the mass of Yparticle material after the conditioning material has been added 'and removing volatiles from the material by passing heated dry air through the vessel in which the material is'conflned. Y v

19. The method ofmaking molding material rin particle form capable of being transformed into a cohesive product by application of heat and pressure which includes the steps of introducing a mass of plasticizable base vmaterial in substantially dry particle form into a .suitable vessel, tumbling the mass within the vessel, introducing plasticizer in fluid form into said vessel. and spraying substantially all of the plus ticizer introduced directly onto the surface of said mass while the mass is-being tumbled and while maintaining said mass in its substantially dry l particle form to thereby cause the uid to be substantially uniformly distributed throughout ticles of the action.

2o. The method .ofmakmg molding material in particle form capable of being transformed into a cohesive product by application of heat and pressure `which includes the steps of introducing a mass of plasticizable base material in` substantially dry particle form into a suitable` vessel, tumbling the mass within the vesselin troducing plasticizer in fluid form into said vessel and intermittently applying substantially all i out the mass by the rubbing contact between the' particles of the mass resulting from the tumbling action. y

a cohesive product by application of heat and pressure which includes the steps of introducing a mass ofl plasticizable base material in substantially dry particle form into a suitable vessel, rotating thevessel to tumble the mass therein, introducing plasticizer in fluid form into said ves- 'sel and intermittently injecting in predetermined timed cycle relation tothe rotation of the vessel substantially all of the plasticizer introduced directly to the surface of the mass while the mass is being tumbled and while maintaining said mass in its substantially dry particle form to thereby cause the uid to be substantially unl-v ,product from molding material in particle,` form which includes the steps of tumbling in a blending vessel a mass of suitable base material in substantially dry particle formfto bring different.

particles to the surface of ythe mass and applying a conditioning material in vfluid form to the surface of the mass while the mass is being tumbled at a rate so related to the rate of tumbling of 17 oi times during the period of such application to change the suriace layer of the mass a multiplicity of times and maintain the mass in itl substantially dry particle form. whereby to eilect substantially uniform distribution of the added huid throughout the substantially dry mass dus to such application of the iiuid to dierently constituted surface layers at diilerent times and the rubbing contact between the particles of the mass during said period and thereafter converting the conditioned substantially dry particle material into a cohesive plastic product by the application of heat and pressure without further treatment after discharge from said blending veel.

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Thafollnwinzreiersncssareoirscordinthe 'meormumenn Um'rnn s'ra'rms rams Number Namo Date 331,242 Hyatt Nov. 24. i888 1,949,434 Schneider Har. 6. im

4.179,200 Great Brits!!! In! 4 im 

